Method of fabricating highly cross-linked polymer spheres having uniform granular sizes
Polymer spheres are fabricated. Dispersing polymerization and a two-stage swelling procedure are processed. The polymer spheres fabricated have uniform granular sizes and are highly cross-linking. Thus, the polymer spheres are heat-resistant and solvent-resistant.
1. A method of fabricating cross-linked polymer spheres having uniform granular sizes, comprising the steps of:
(a) obtaining a plurality of seeds through dispersion polymerization;
(b) mixing a content of a swelling assistant and a content of a surfactant to be added with said plurality of seeds to obtain a seed solution, wherein said swelling assistant, said surfactant and said plurality of seeds are mixed through ultra-sonic vibration with magnetite for 30˜40 minutes (min) and, then, are stirred with a mechanical stirrer at a speed of 120˜160 rounds per minute (rpm) under a temperature of 25˜35 Celsius degrees (° C.) for a time period of 8˜12 hours (hr);
(c) uniformly mixing a content of a monomer and a content of an initiator to be added with a content of a cross-linking agent and a content of a surfactant to obtain a monomer emulsion after homogenization; and
(d) mixing said seed solution and said monomer emulsion to be stirred and added with a stabilizer and an inhibitor after processing monomer swelling; then, flowing in nitrogen and stirring to uniformly process mixing; and, then, heating up to process polymerization to obtain a plurality of cross-linked polymer spheres, wherein said spheres have an average granular diameter twice as big as that of said seeds.
2. The method according to claim 1 , wherein, in step (a), on obtaining said plurality of seeds, a stabilizer is added into a solvent, stirred with magnetite and purged with nitrogen to obtain a first mixed solution; then, said first mixed solution is added with a monomer and an initiator, and purged with nitrogen to obtain a second mixed solution; then, said second mixed solution is put in a water batch to obtain an emulsion having uniform submicrospheres; and, then, said emulsion is processed through repeated centrifugal washing with water and methanol to obtain said plurality of seeds after removing leftover monomers and stabilizer.
3. The method according to claim 1 , wherein step (b) to (d) are a two-stage swelling procedure.
4. The method according to claim 1 , wherein, in step (b), said swelling assistant is cyclohexane.
5. The method according to claim 1 , wherein, in step (b), said surfactant is sodium dodecyl sulfate (SDS) having a concentration of 0.25 percents (wt %) and a dose of 40˜60 grams (g).
6. The method according to claim 1 , wherein, in step (b), said plurality of seed has a dose of 0.1˜0.2 g.
7. The method according to claim 1 , wherein, in step (c), said monomer is methyl methacrylate (MMA).
8. The method according to claim 1 , wherein, in step (c), said initiator is benzoyl peroxide (BPO).
9. The method according to claim 1 , wherein, in step (c), said cross-linking agent is ethylene glycol dimethacrylate (EGDMA) and is added at a concentration of 15˜25 wt %.
10. The method according to claim 1 , wherein, in step (c), said surfactant is sodium dodecyl sulfate (SDS) having a concentration of 0.25 wt % and a dose of 90˜120 g.
11. The method according to claim 1 , wherein, in step (d), said monomer swelling is processed at a temperature of 25˜40° C. and, then, is stirred with a mechanical stirrer at a speed of 120˜160 rpm for 5˜8 hrs to mix said seed solution and said monomer emulsion.
12. The method according to claim 1 , wherein, in step (d), said stabilizer is polyvinyl alcohol (PVA) having a concentration of 4˜6 wt %.
13. The method according to claim 1 , wherein, in step (d), said inhibitor is sodium nitrite (NaNO 2 ) having a dose of 0.1˜0.2 g.
14. The method according to claim 1 , wherein, in step (d), after flowing in nitrogen, a mechanical stirrer is used to process uniform mixing by stirring at a speed of 120˜160 rpm for 25˜40 min.
15. The method according to claim 1 , wherein, in step (d), after increasing temperature to 65˜80° C., said polymerization is processed for 9˜12 hrs to obtain said plurality of polymer spheres having an average granular diameter twice as big as that of said seeds.
16. The method of claim 1 , wherein the diameter of said spheres is between about 5.1 and about 5.2 μm.
17. A method of fabricating cross-linked polymer spheres having uniform granular sizes, comprising the steps of:
(a) obtaining a plurality of seeds through dispersion polymerization;
(b) mixing a content of a swelling assistant and a content of a surfactant to be added with said plurality of seeds to obtain a seed solution;
(c) uniformly mixing a content of a monomer and a content of an initiator to be added with a content of a cross-linking agent and a content of a surfactant to obtain a monomer emulsion after homogenization, wherein said monomer, said initiator, said cross-linking agent and said surfactant are homogenized at a speed of about 8000 to about 12,000 rpm for 10˜20 min and, then, are uniformly dispersed with a ultra-sonic shaker for 10˜20 min to obtain said monomer emulsion;
(d) mixing said seed solution and said monomer emulsion to be stirred and added with a stabilizer and an inhibitor after processing monomer swelling; then, flowing in nitrogen and stirring to uniformly process mixing; and, then, heating up to process polymerization to obtain a plurality of cross-linking polymer spheres, wherein said spheres have an average granular diameter twice as big as that of said seeds.